Development of a gas chromatography/mass spectrometry method to quantify several urinary monohydroxy metabolites of polycyclic aromatic hydrocarbons in occupationally exposed subjects.
The aim of this study was the development of a method for the determination of 12 urinary monohydroxy metabolites of PAHs, namely 1-hydroxynaphthalene, 2-hydroxynaphthalene, 2-hydroxyfluorene, 9-hydroxyfluorene, 1-hydroxyphenanthrene, 2-hydroxyphenanthrene, 3-hydroxyphenanthrene, 4-hydroxyphenanthrene, 9-hydroxyphenanthrene, 1-hydroxypyrene, 6-hydroxychrysene, and 3-hydroxybenzo[a]pyrene. Analytes were determined in the presence of deuterated analogues as internal standards, by GC/MS operating in the electron impact mode. Sample preparation was performed by enzymatic hydrolysis of glucoronate and sulphate conjugates of hydroxy metabolites of PAHs, liquid-liquid extraction with n-hexane, and derivatization with a silylating reagent. The method is very specific, limits of quantification are in the range 0.1-1.4 microg/l, and range of linearity is from limit of detection to 208 microg/l. Within- and between-run precision, expressed as coefficient of variation, are <20%; accuracy for most analytes is within 20% of the theoretical value. An application of the proposed method to the analysis of 10 urine samples from coke-oven workers shows that 1-hydroxynaphthalene and 2-hydroxyfluorene were the most abundant compounds (median 61.4 and 69.7 microg/l, respectively), while 6-hydroxychrysene, and 3-hydroxybenzo[a]pyrene were always below the quantification limit.
Campo
Laura
L
Department of Occupational and Environmental Health, University of Milan, Milan, Italy. laura.campo@unimi.it
Rossella
Federica
F
Fustinoni
Silvia
S
D002911:Chrysenes / Q000378:metabolism / Q000652:urine; D004355:Drug Stability; D004784:Environmental Monitoring / Q000379:methods*; D005449:Fluorenes / Q000378:metabolism / Q000652:urine; D008401:Gas Chromatography-Mass Spectrometry / Q000379:methods*; D006801:Humans; D016014:Linear Models; D008297:Male; D009284:Naphthols / Q000378:metabolism / Q000652:urine; D016273:Occupational Exposure / Q000032:analysis; D010616:Phenanthrenes / Q000378:metabolism / Q000652:urine; D011084:Polycyclic Aromatic Hydrocarbons / Q000378:metabolism* / Q000652:urine*; D011721:Pyrenes / Q000032:analysis / Q000378:metabolism; D012015:Reference Standards; D015203:Reproducibility of Results; D012680:Sensitivity and Specificity
D002911:Chrysenes; D005449:Fluorenes; D009284:Naphthols; D010616:Phenanthrenes; D011084:Polycyclic Aromatic Hydrocarbons; D011721:Pyrenes; C087203:6-hydroxychrysene; C033146:1-hydroxypyrene